A newly developed countercurrent chromatographic (CCC) scheme yields a highly efficient preparative-scale separations in a short periof of time ranging 2-5 hours. The method uses a coil planet centrifuge which produces a synchronous planetary motion of the holder. The column consists of multiple layers of the coil called "multi-layer coil", which is accommodated on a spool-shaped column holder. The system produces excellent retention of the stationary phase against a high flow of the mobile phase. Consequently, solutes locally introduced at the inlet of the column are efficiently separated according to their particion coefficient in the manner analogous to the liquid partition chromatography but in the absence of solid supports. The capability of the present method has been demonstrated on separation of various biological materials which include DNP amino acids, natural and synthetic peptides, indole plant hormones, purines and pyrimidines, etc.